1-Chloro-3-phenoxy-2-propanol → 7-[3-(3-Phenoxy-2-hydroxypropylamino)-propyl]-theophylline

HRID 614326

반응식

HRID 614326 반응식
[NH2:1][CH2:2][CH2:3][CH2:4][N:5]1[C:14]2[C:13](=[O:15])[N:11]([CH3:12])[C:10](=[O:16])[N:9]([CH3:17])[C:8]=2[N:7]=[CH:6]1.Cl[CH2:19][CH:20]([OH:29])[CH2:21][O:22][C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1>C(O)C>[O:22]([CH2:21][CH:20]([OH:29])[CH2:19][NH:1][CH2:2][CH2:3][CH2:4][N:5]1[C:14]2[C:13](=[O:15])[N:11]([CH3:12])[C:10](=[O:16])[N:9]([CH3:17])[C:8]=2[N:7]=[CH:6]1)[C:23]1[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=1

참가 물질

4

반응물 2

HCID 943001-Chloro-3-phenoxy-2-propanolHCID 29652267-(3-aminopropyl)-1,3-dimethyl-3,7-dihydro-1H-purine-2,6-dione

생성물 1

HCID 213292787-[3-(3-Phenoxy-2-hydroxypropylamino)-propyl]-theophylline

시약·촉매·용매 1

HCID 702Ethanol용매

실험 절차

A mixture of 75 g of 7-(3-aminopropyl)-theophylline and 27.4 g of 1-chloro-3-phenoxy-2-propanol is heated for 8 hours at 130° to 140° C. After the melt has been cooled to 70°-90° C., ethanol is added to it, followed by brief boiling under reflux. After standing overnight, the untreated and precipitated aminopropyl theophylline hydrochloride is filtered off under suction, the filtrate is acidified with alcoholic hydrochloric acid, heavily concentrated and acetone added until crystallisation begins. The reaction product then separates and is recrystallised from methanol. Yield 30.2 g. Melting point of the hydrochloride: 183°-186° C.

후처리

  1. temperatureis heated for 8 hours at 130° to 140° C
  2. temperatureAfter the melt has been cooled to 70°-90° C.
  3. temperatureunder reflux
  4. customthe untreated and precipitated aminopropyl theophylline hydrochloride
  5. filtrationis filtered off under suction
  6. concentrationheavily concentrated
  7. additionacetone added until crystallisation
  8. customis recrystallised from methanol
  9. custom183°-186° C.

출처 및 근거

ORD 기록
ord-efeded0832d9465981883351326e06bc
출처 데이터셋
uspto-grants-1979_03
특허 번호
US04144340

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